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Here we present a systematic analysis of the synthesis of unsymmetrical disulphides employing 6‐thioguanosine and its mono‐ and dinucleotides by three of the most common strategies: a nucleophilic substitution of the thiol, a thiol exchange reaction with another disulphide and oxidative dehydrogenation coupling reactions of S−H bonds. The exchange reaction was found to be the most efficient approach...